CN106831402A - A kind of process for purification of sodium citrate - Google Patents
A kind of process for purification of sodium citrate Download PDFInfo
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- CN106831402A CN106831402A CN201611211401.7A CN201611211401A CN106831402A CN 106831402 A CN106831402 A CN 106831402A CN 201611211401 A CN201611211401 A CN 201611211401A CN 106831402 A CN106831402 A CN 106831402A
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- China
- Prior art keywords
- sodium citrate
- purification
- sodium
- citric acid
- water
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- 238000000034 method Methods 0.000 title claims abstract description 30
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 title claims abstract description 30
- 239000001509 sodium citrate Substances 0.000 title claims abstract description 29
- 238000000746 purification Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000047 product Substances 0.000 claims abstract description 23
- OAGSFHDUINSAMQ-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;sodium;hydrate Chemical compound O.[Na].OC(=O)CC(O)(C(O)=O)CC(O)=O OAGSFHDUINSAMQ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 21
- 239000012043 crude product Substances 0.000 claims abstract description 13
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 230000006837 decompression Effects 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical class O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002932 luster Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000006641 stabilisation Effects 0.000 abstract description 3
- 238000011105 stabilization Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 235000005979 Citrus limon Nutrition 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 206010023126 Jaundice Diseases 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 229940127219 anticoagulant drug Drugs 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000007844 bleaching agent Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of process for purification of sodium citrate, the method comprises the following steps：（1）Two citric acid monohydrate sodium crude products are carried out into Pressurized-heated dissolving with a small amount of water, sodium citrate aqueous solution is obtained；（2）With step（1）Filtered under same pressure condition, slowly depressurize crystallisation by cooling；（3）Separation of solid and liquid, obtains solids；（4）It is dried during solids is sent into vacuum rotating drier, obtains two citric acid monohydrate sodium finished products.The present invention has advantages below：Production process is easy to control, and operating process is simple, and the sodium citrate purity prepared using the method is high, and yield is high, and color and luster is pure white, and impurity is few, product quality stabilization.
Description
Technical field
The present invention is a kind of method of purification of chemicals, specifically a kind of process for purification of sodium citrate.
Background technology
Trisodium citrate dihydrate is white powdered, as food additives, electroplating industry complexing agent, buffer,
Medical industry is used to manufacture anticoagulant medicine, and light industry is used as auxiliary agent of detergent etc..Stabilization in normal temperature and air, in humid air
In it is micro- have dissolubility, in hot-air produce weathering phenomenon.It is heated to 150 DEG C and loses the crystallization water.The lemon high in order to obtain purity
Lemon acid sodium, it is common practice to dissolve, filter, decolourizing, normal temperature and pressure is concentrated, crystallizing, dry；But resulting coloured product
Jaundice, this is had a greatly reduced quality for the quality of product, and yield is low and produces a large amount of mother liquors, and such as fruit mother liquor reuse can be caused into
Product are further turned to be yellow, such as fruit mother liquor not reuse, and raw material can be wasted again, produce substantial amounts of organic liquid waste, pollute environment.《Salt
City engineering college journal》Volume 23 the 1st interim one, 03 month 2010 bottom on《The application of sodium citrate and preparation method research》One
The article pointed out, sodium citrate has good water solubility that there is excellent chelating energy to metal ions such as the calcium ion in water, magnesium ions
Power；And at the end of sodium citrate feeds intake, the pH value of reaction solution must be controlled more than 10.0；For solution ph before concentration
Adjustment in, experiment shows, the pH value of solution directly affects product quality before concentration distillation, and then solution ph is with distillation
It is continually changing, it is difficult to control, the product acid-base value that crystallization is obtained is extremely unstable, therefore regulation and control pH value is crucial one of comparing
Step.It is also strict control, the product colour for otherwise obtaining for the consumption of the bleaching agent activated carbon employed in decolorization process
For light yellow or slightly yellow.
The content of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of simple to operate, color and luster it is pure white, rate
The process for purification of sodium citrate high.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of process for purification of sodium citrate, should
Method comprises the following steps：
（1）Two citric acid monohydrate sodium crude products are carried out into Pressurized-heated dissolving with a small amount of water, sodium citrate aqueous solution is obtained；
（2）With step（1）Filtered under same pressure condition, slowly depressurize crystallisation by cooling；
（3）Separation of solid and liquid, obtains solids；
（4）It is dried during solids is sent into vacuum rotating drier, obtains two citric acid monohydrate sodium finished products.
Further, the two citric acid monohydrates sodium crude product and the mass ratio of water are 10 ~ 12:1, the water is deionization
Water.Using deionized water, it is possible to reduce the foreign ion in final product.
Further, step（1）In, pressure is 1 ~ 2MPa.
Further, step（1）In, temperature is 60 ~ 80 DEG C.
Further, step（2）In, slowly the step of decompression is：According to subtracting 0.01 per hour ~ 0.02MPa.
Further, step（4）In, dry vacuum is -0.09 ~ -0.08MPa, 50 ~ 70 DEG C of temperature, drying time
It is 3 ~ 6h.
Beneficial effect：Compared with prior art, the present invention has advantages below：Production process is easy to control, operating process letter
Single, the sodium citrate purity prepared using the method is high, and yield is high, and color and luster is pure white, and impurity is few, product quality stabilization, waste liquid amount
It is few.
Specific embodiment
Below by specific embodiment, the present invention is further described, it is noted that for the ordinary skill of this area
For personnel, under the premise without departing from the principles of the invention, some variations and modifications can also be made, these also should be regarded as belonging to
Protection scope of the present invention.
Embodiment 1：A kind of process for purification of sodium citrate, the method comprises the following steps：
（1）Two citric acid monohydrate sodium crude products are carried out into Pressurized-heated dissolving with a small amount of water, sodium citrate aqueous solution is obtained；Wherein,
Two citric acid monohydrate sodium crude products are 10 with the mass ratio of water:1, the water is deionized water；Pressure is 1MPa, and temperature is 60 DEG C；
（2）With step（1）Filtered with bag type filtering machine under the conditions of same pressure and temp, then slow decompression cooling is tied again
It is brilliant；The step of slow decompression is：According to subtracting 0.02MPa per hour；
（3）After reducing to normal pressure, separation of solid and liquid obtains solids；
（4）Will solids send into vacuum rotating drier in be dried, dry vacuum be -0.08MPa, temperature 70 C,
Drying time is 6h；Obtain two citric acid monohydrate sodium finished products, yield 87.4%.
After two citric acid monohydrate sodium finished products are detected through the detection method of GB6782-86, its content is 99.95%；Color and luster is clean
In vain, finished product is in crystalline powder.
Embodiment 2：A kind of process for purification of sodium citrate, the method comprises the following steps：
（1）Two citric acid monohydrate sodium crude products are carried out into Pressurized-heated dissolving with a small amount of water, sodium citrate aqueous solution is obtained；Wherein,
Two citric acid monohydrate sodium crude products are 12 with the mass ratio of water:1, the water is deionized water；Pressure is 2MPa, and temperature is 80 DEG C；
（2）With step（1）Carry out being filtered with bag type filtering machine under the conditions of same pressure and temp, then slow decompression cooling again
Crystallization；The step of slow decompression is：According to subtracting 0.01MPa per hour；
（3）After reducing to normal pressure, separation of solid and liquid obtains solids；
（4）Will solids send into vacuum rotating drier in be dried, dry vacuum be -0.09MPa, temperature 50 C,
Drying time is 3h；Obtain two citric acid monohydrate sodium finished products, yield 93.2%.
After two citric acid monohydrate sodium finished products are detected through the detection method of GB6782-86, its content is 99.93%；Color and luster is clean
In vain, finished product is in crystalloid.
Embodiment 3：A kind of process for purification of sodium citrate, the method comprises the following steps：
（1）Two citric acid monohydrate sodium crude products are carried out into Pressurized-heated dissolving with a small amount of water, sodium citrate aqueous solution is obtained；Wherein,
Two citric acid monohydrate sodium crude products are 11 with the mass ratio of water:1, the water is deionized water；Pressure is 1.5MPa, and temperature is 70
℃；
（2）With step（1）Carry out being filtered with bag type filtering machine under the conditions of same pressure and temp, then slow decompression cooling again
Crystallization；The step of slow decompression is：According to subtracting 0.015MPa per hour；
（3）After reducing to normal pressure, separation of solid and liquid obtains solids；
（4）Will solids send into vacuum rotating drier in be dried, dry vacuum be -0.083MPa, temperature 60 C,
Drying time is 5h；Obtain two citric acid monohydrate sodium finished products, yield 91.8%.
After two citric acid monohydrate sodium finished products are detected through the detection method of GB6782-86, its content is 99.97%；Color and luster is clean
In vain, finished product is in crystalloid.
Embodiment 4：A kind of process for purification of sodium citrate, the method comprises the following steps：
（1）Two citric acid monohydrate sodium crude products are carried out into Pressurized-heated dissolving with a small amount of water, sodium citrate aqueous solution is obtained；Wherein,
Two citric acid monohydrate sodium crude products are 10.8 with the mass ratio of water:1, the water is deionized water；Pressure is 1.3MPa, and temperature is 65
℃；
（2）With step（1）Carry out being filtered with bag type filtering machine under the conditions of same pressure and temp, then slow decompression cooling again
Crystallization；The step of slow decompression is：According to subtracting 0.012MPa per hour；
（3））After reducing to normal pressure, separation of solid and liquid obtains solids；
（4）Will solids send into vacuum rotating drier in be dried, dry vacuum be -0.088MPa, temperature 60 C,
Drying time is 4h；Obtain two citric acid monohydrate sodium finished products, yield 90.6%.
After two citric acid monohydrate sodium finished products are detected through the detection method of GB6782-86, its content is 99.96%；Color and luster is clean
In vain, finished product is in crystalloid.
Claims (7)
1. a kind of process for purification of sodium citrate, it is characterised in that the method comprises the following steps：
（1）Two citric acid monohydrate sodium crude products are carried out into Pressurized-heated dissolving with a small amount of water, sodium citrate aqueous solution is obtained；
（2）With step（1）Filtered under same pressure condition, slowly depressurize crystallisation by cooling；
（3）Separation of solid and liquid, obtains solids；
（4）It is dried during solids is sent into vacuum rotating drier, obtains two citric acid monohydrate sodium finished products.
2. a kind of process for purification of sodium citrate according to claim 1, it is characterised in that the two citric acid monohydrates sodium
Crude product is 10 ~ 12 with the mass ratio of water:1.
3. the process for purification of a kind of sodium citrate according to claim 1, it is characterised in that the water is deionized water.
4. a kind of process for purification of sodium citrate according to claim 1, it is characterised in that step（1）In, pressure be 1 ~
2MPa。
5. a kind of process for purification of sodium citrate according to claim 1, it is characterised in that step（1）In, temperature is 60
~80℃。
6. a kind of process for purification of sodium citrate according to claim 1, it is characterised in that step（2）In, slow decompression
The step of be：According to subtracting 0.01 per hour ~ 0.02MPa.
7. a kind of process for purification of sodium citrate according to claim 1, it is characterised in that step（4）In, it is dry true
Reciprocal of duty cycle is -0.09 ~ -0.08MPa, and 50 ~ 70 DEG C of temperature, drying time is 3 ~ 6h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611211401.7A CN106831402A (en) | 2016-12-24 | 2016-12-24 | A kind of process for purification of sodium citrate |
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| CN201611211401.7A CN106831402A (en) | 2016-12-24 | 2016-12-24 | A kind of process for purification of sodium citrate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108865473A (en) * | 2018-06-27 | 2018-11-23 | 合肥同佑电子科技有限公司 | A kind of scale remover and preparation method thereof for computor-keyboard |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3886069A (en) * | 1972-11-24 | 1975-05-27 | Olav Erga Trondheim | Process for purification of aqueous sodium citrate solutions |
| CN102659566A (en) * | 2012-04-11 | 2012-09-12 | 湖南华日制药有限公司 | Production technology of medicinal anhydrous citric acid |
| CN104262139A (en) * | 2014-08-28 | 2015-01-07 | 华北制药集团先泰药业有限公司 | Preparation method of sodium citrate crystal through solvent-out crystallization |
| CN105037140A (en) * | 2015-06-26 | 2015-11-11 | 宁乡新阳化工有限公司 | Anhydrous sodium citrate production method |
-
2016
- 2016-12-24 CN CN201611211401.7A patent/CN106831402A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3886069A (en) * | 1972-11-24 | 1975-05-27 | Olav Erga Trondheim | Process for purification of aqueous sodium citrate solutions |
| CN102659566A (en) * | 2012-04-11 | 2012-09-12 | 湖南华日制药有限公司 | Production technology of medicinal anhydrous citric acid |
| CN104262139A (en) * | 2014-08-28 | 2015-01-07 | 华北制药集团先泰药业有限公司 | Preparation method of sodium citrate crystal through solvent-out crystallization |
| CN105037140A (en) * | 2015-06-26 | 2015-11-11 | 宁乡新阳化工有限公司 | Anhydrous sodium citrate production method |
Non-Patent Citations (1)
| Title |
|---|
| 叶铁林: "《化工结晶过程原理及应用》", 31 December 2006 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108865473A (en) * | 2018-06-27 | 2018-11-23 | 合肥同佑电子科技有限公司 | A kind of scale remover and preparation method thereof for computor-keyboard |
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Application publication date: 20170613 |